分散液液微萃取-气相色谱/质谱法测定松茸中18种邻苯二甲酸酯

目的 建立松茸中18种邻苯二甲酸酯类（PAEs）的分散液液微萃取-气相色谱/质谱分析方法（DLLME-GC/MS），并用于松茸中邻苯二甲酸酯的污染调查。方法 样品经乙腈超声提取后，经三氯甲烷分散液液微萃取，氮吹干、甲醇复溶后进样测定，内标法定量。结果 方法线性范围为0.001～1.00mg/L（DBEP和DCHP为0.005～1.00mg/L），相关系数均大于0.9995。方法检出限为0.10～0.85μg/kg,定量限为0.33～2.84μg/kg。在3个加标浓度水平下的加标回收率为80.23%～118.0%，相对标准偏差为1.38%～14.7%。用本法检测了18个松茸样品，检出多种PAEs，总含量范围（∑PAEs）为12.62~5430μg/kg。结论 该方法具有简单、快速、灵敏、价廉等优点，适用于松茸中18种邻苯二甲酸酯的测定。

Determination of 18 phthalate acid esters in matsutake by dispersive liquid-liquid microextraction-gas chromatography/mass spectrometry

To establish a method for the determination of 18 phthalate acid esters(PAEs) in matsutake by dispersive liquid-liquid microextraction-gas chromatography-mass spectrometry(DLLME-GC/MS), and to investigate the contamination status of PAEs in matsutakes. Methods PAEs in samples were extracted by ultrasound with acetonitrile, and then liquid-liquid microextracted with trichloromethane which was taken and dried-up under nitrogen gas, finally the residue was dissolved with methanol, and the solution was injected to GC/MS for analysis. The quantification was based on the internal standard curves. Results The linear ranges of the method were 0.001-1.00 mg/L(DBEP and DCHP were 0.005-1.00 mg/L), with the correlation coefficients all greater than 0.9995. The limits of detection(LODs) was 0.10-0.85 μg/kg and the limits of quantification(LOQs) was 0.33-2.84 μg/kg. The recoveries were 80.23%-118.0 % and the relative standard deviations(RSDs) were 1.38%-14.69%. Some of PAEs were detected in 18 matsutake samples by this method and the total contents of PAEs ranged from 12.62 to 5 430 g/kg. Conclusion The method is simple, rapid, sensitive and cheap. And it is suitable for simultaneous determination of 18 PAEs in matsutake.